Gas chromatographic, high performance liquid chromatographic and GC-io
n trap detector mass spectrometric analyses of the hydroperoxides form
ed during thermal peroxidation of cholesteryl acetate, are reported an
d discussed. The hydroperoxides were separated from the thermal-oxidis
ed mixture by solid-phase extraction, fractionated and individually co
llected by HPLC. Each hydroperoxide was then chemically reduced with N
aBH4 to a hydroxy-derivative. The GC and MS characteristics of hydroxy
- and TMS-derivatives were compared against available standards. Only
7 beta-hydroperoxide and 7 alpha-hydro-peroxide of cholesteryl acetate
were found, as reported in the literature for cholesterol.